CN103396119A - Preparation method of single-phase pyrochlore-type La2Zr2O7 nano-powder - Google Patents
Preparation method of single-phase pyrochlore-type La2Zr2O7 nano-powder Download PDFInfo
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- CN103396119A CN103396119A CN2013103727032A CN201310372703A CN103396119A CN 103396119 A CN103396119 A CN 103396119A CN 2013103727032 A CN2013103727032 A CN 2013103727032A CN 201310372703 A CN201310372703 A CN 201310372703A CN 103396119 A CN103396119 A CN 103396119A
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Abstract
The invention relates to a preparation method of single-phase pyrochlore-type La2Zr2O7 nano-powder. The preparation method is characterized in that the La2Zr2O7 nano-powder is obtained by ageing, drying and high-temperature roasting by using Zr<4+> and La<3+> hydration inorganic salt as a precursor, citric acid as a complexing agent, an amide organic matter as a gel accelerant and polyethylene glycol as a dispersing agent. The single-phase pyrochlore-type La2Zr2O7 nano-powder has the advantages that the particle size of the obtained La2Zr2O7 nano-powder is 20-100nm, the molar ratio of Zr to La is approximate to 1:1, the crystal structure of the La2Zr2O7 nano-powder is single-phase pyrochlore-type, and the La2Zr2O7 nano-powder has high degree of crystallinity and excellent performances such as low heat conduction, sintering resistance, good high-temperature stability and the like and is applied to the field of thermal barrier coatings of aviation turbine engines and protective coatings in high-temperature wet-oxygen environments.
Description
Technical field
The present invention relates to a kind of preparation method of single-phase RE oxide ceramics superfine powder, particularly relate to sol-gel method and prepare single-phase pyrochlore-type La
2Zr
2O
7Nano-powder.
Background technology
Along with fuel gas temperature and the pressure of aero-turbine improves constantly, traditional thermal structure alloy can't satisfy the demands, and improving stability and the service life of material under higher temperature is problem in the urgent need to address.At present, the surface temperature that thermal barrier coating (TBCs) technology is passed through to reduce bulk material, to improve the engine service life, has become the focus of current research.Usually the method that prepare TBCs has plasma spraying method, electro beam physics vapour deposition method, chemical Vapor deposition process and lf method etc., wherein, develop comparative maturity, most widely used be plasma spraying method, its raw material is powder body material.Zirconic acid lanthanum (La
2Zr
2O
7) be a kind of material of pyrochlore constitution, have lower thermal conductivity, below fusing point without the excellent properties such as phase transformation, Heat stability is good as in the preferred powder body material that uses under high temperature, and prepare that single crystalline phase, degree of crystallinity are high, good dispersity, La that granularity is little
2Zr
2O
7Powder is to affect plasma spray La
2Zr
2O
7The key of coating performance.
Preparation La commonly used
2Zr
2O
7The method of powder is solid phase method, but solid reaction process synthesis temperature higher (1550～1650 ℃) is difficult to controlling composition and crystallization phases, and the La that obtains of solid phase method
2Zr
2O
7Powder grain size is large, size distribution is inhomogeneous, and this has just limited its application at high temperature.Liquid preparation methods La
2Zr
2O
7Advantage be: precursor is mixed with molecular level, thereby the powder granule that finally obtains is less and be uniformly dispersed.More ripe liquid phase preparation technology is coprecipitation method at present, and patent CN101407336A discloses a kind of La
2Zr
2O
7The co-precipitation preparation method of powder, will contain Zr
4+And La
3+Two kinds of precursor solutions mix, add precipitation agent to generate precipitation, obtain La through washing, high-temperature roasting
2Zr
2O
7Powder, the powder granule degree that this method obtains is large, and contains the impurity phase fluorite structure in structure.
Sol-gel method belongs to the liquid phase method category, compares preparation La with traditional coprecipitation method
2Zr
2O
7Powder granule is less, can reach nanometer level, and phase consists of single pyrrhite phase, and uniform particles and purity are high, have the advantages such as anti-sintering, high-temperature-phase good stability, physical strength height, are more suitable for the powder body material as plasma spraying TBCs.Document 1 " Liu Shuxin, Haibin Wang. original position is synthesized La
2Zr
2O
7-YSZ matrix material and high-temperature thermal stability Journal of Sex Research, Chinese powder technology, 2011,17 (4): 65-70. " announced a kind of La
2Zr
2O
7The sol-gel process for preparing of-YSZ powder, it adopts metal nitrate as raw material, and citric acid has prepared La as complexing agent
2Zr
2O
7-YSZ powder, but owing to not adding dispersion agent, the particle size of gained powder is larger, reaches micron order.Document 2 " Vladimir Sevast ' yanov, Elizaveta Simonenko, Nikolai Simonenko, et al.Synthesis of finely dispersed La
2Zr
2O
7, La
2Hf
2O
7, Gd
2Zr
2O
7And Gd
2Hf
2O
7Oxides.Mendeleev Commun., 2013,23:17-18. " adopt metal inorganic salt as raw material, add concentrated nitric acid, citric acid, ethylene glycol, adopt ammoniacal liquor to regulate the pH value, prepare La
2Zr
2O
7Nano-powder, still can't slowly control the variation of pH value due to ammoniacal liquor, colloidal solid is difficult to evenly grow up, thereby causes crystallinity poor.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, solve existing sol-gel method and prepare La
2Zr
2O
7The problem such as powder high-temperature stability deficiency, easy-sintering, physical strength are not high, provide that a kind of single crystalline phase, degree of crystallinity are high, good dispersity, La that granularity is little
2Zr
2O
7Powder preparation method.
The present invention is achieved through the following technical solutions:
1, preparation precursor solution:
Adopt metal hydration inorganic salt as precursor, adopt the mixed solution of water and alcohol as solvent, will contain Zr
4+And La
3+Hydrated inorganic salt slowly join respectively in the mixed solution of water and alcohol, continue stirring and dissolving, obtain two kinds of precursor solutions, each component molar content ratio is respectively: Zr
4+: H
2O: alcohol=1:5～8:10, La
3+: H
2O: alcohol=1:0.5～2:10;
Wherein, contain Zr
4+Hydrated inorganic salt be ZrOCl
28H
2O or Zr (NO
3)
45H
2O, contain La
3+Hydrated inorganic salt be La (NO
3)
36H
2O or LaCl
36H
2O, alcoholic solvent are methyl alcohol, ethanol or propyl alcohol, preferred alcohol;
2, prepare colloidal sol:
Two kinds of solution of step 1 gained are pressed component mol ratio Zr
4+: La
3+=1:1 mixes and continues stirring, adds successively citric acid, and mol ratio is citric acid: Zr
4+=0.1～0.4:1; Add polyoxyethylene glycol constituent mass ratio to be: polyoxyethylene glycol: Zr
4+=1:1～7.5, wherein, the number-average molecular weight of polyoxyethylene glycol can be 600～20000; Add methane amide or N-METHYLFORMAMIDE, mol ratio is: methane amide or N-METHYLFORMAMIDE: Zr
4+=0.1～2:1, continue to stir 1～5h with above-mentioned mixed solution, forms colloidal sol;
3, aging:
Colloidal sol is incubated aging under 60～90 ℃, continues 10～24h, obtain wet gel; Selection process is the aging 15h of insulation under 80 ℃ of conditions, and aging temperature is higher, and digestion time shortens relatively;
4, drying:
100～200 ℃ of dryings, be 5～10h time of drying, obtains xerogel with wet gel; Selection process is dry 6h under 120 ℃ of conditions, and drying temperature is higher, and relatively shorten time of drying;
5, high-temperature roasting:
Xerogel is incubated 1～5h again after the temperature rise rate of 1～10 ℃/min rises to 1000～1200 ℃,, with the stove cooling, obtains La
2Zr
2O
7Powder, selection process are that 5 ℃/min rises to 1200 ℃, and insulation 2h, lower the temperature with stove.
The present invention is a kind of improved sol-gel process for preparing, with traditional sol-gel method, compares, and precursor used reduces greatly than traditional metal alkoxide cost, and citric acid strengthens the colloid network as complexing agent; Adopt polyoxyethylene glycol as dispersion agent, polyoxyethylene glycol has the characteristic of tensio-active agent, can make the colloidal solid of containing metal-oxygen key even at solvent dispersion, reduces the size of gelation gained micelle, finally reduces the granular size of gained powder; Adopt amides additive control gelation process, the amides additive is through being hydrolyzed the H that can remove in solution
+, improve the pH value of solution, the effect that this process is regulated pH value than strong alkaline substances such as ammoniacal liquor slowly many, thereby can guarantee colloidal solid slowly, the even growth, the network structure that full cross-linked formation is good, obtain the good La of crystallinity after high-temperature roasting
2Zr
2O
7Powder.The method technique is simple, cost is low, corrosion-free to equipment, prepared powder is that single pyrrhite phase, elementary composition near stoichiometric proportion, good crystallinity, granular size are nano level, are uniformly dispersed.
Raw material required for the present invention all can obtain by open channel from market, and testing installation is common equipment.
Description of drawings
Fig. 1 is the La of the embodiment of the present invention 1 preparation
2Zr
2O
7The SEM photo of powder;
Fig. 2 is the La of the embodiment of the present invention 1 preparation
2Zr
2O
7The TEM photo of powder;
Fig. 3 is the La of the embodiment of the present invention 1 preparation
2Zr
2O
7The XRD spectra of powder;
Fig. 4 is the La of the embodiment of the present invention 3 preparations
2Zr
2O
7The SEM photo of powder;
Fig. 5 is the La of the embodiment of the present invention 3 preparations
2Zr
2O
7The TEM photo of powder;
Fig. 6 is the La of the embodiment of the present invention 3 preparations
2Zr
2O
7The XRD spectra of powder;
Embodiment
The invention will be further described by the following examples, but protection domain is not subjected to the restriction of these embodiment.Should be understood that in addition after having read content of the present invention, those skilled in the art can make various changes or modifications the present invention, these equivalent form of values fall within appended claims limited range of the present invention equally.
Embodiment 1
A kind of single-phase pyrochlore-type La of the present invention's preparation
2Zr
2O
7Nano-powder mainly contains following steps:
(1) ZrOCl in molar ratio
28H
2O:H
2O:CH
3OH=1:5:10, with 5.00g ZrOCl
28H
2O slowly joins in the mixed solution of 1.40g water and 4.97g methyl alcohol, constantly stirs, and obtains clear solution A liquid; Simultaneously, La (NO in molar ratio
3)
36H
2O:H
2O:CH
3OH=1:0.5:10, with 6.66g La (NO
3)
36H
2O slowly adds in the mixed solution of 0.14g water and 4.97g methyl alcohol, constantly stirs, and obtains clear solution B liquid;
(2) A liquid and B liquid are mixed, obtain transparent mixing solutions, stir;
(3) under the condition that continue to stir, successively in mixed solution in molar ratio: citric acid: Zr
4+=0.1:1 adds citric acid 0.33g, polyoxyethylene glycol in mass ratio: Zr
4+=1:1 adds polyoxyethylene glycol 1.41g, and wherein, the number-average molecular weight of polyoxyethylene glycol is 600, in molar ratio N-METHYLFORMAMIDE: Zr
4+=0.1:1 adds N-METHYLFORMAMIDE 0.09g, stirs 1h, obtains colloidal sol;
(4) with colloidal sol at 60 ℃ of aging 24h, then through 100 ℃ of dry 10h, obtain faint yellow xerogel;
(5) xerogel is risen to 1000 ℃ through 1 ℃/min in retort furnace, then be incubated 5h,, with the stove cooling, obtain La
2Zr
2O
7Powder.
The present embodiment gained La
2Zr
2O
7As shown in Figure 1, visible gained powder is uniformly dispersed the SEM photo of powder; The present embodiment gained La
2Zr
2O
7As shown in Figure 2, the particle size of visible powder is nano level, approximately 40～100nm to the TEM photo of powder; The present embodiment gained La
2Zr
2O
7As shown in Figure 3, the phase composite of visible powder is single for the XRD spectra of powder, and structure is pyrochlore-type, and crystallinity is good.
A kind of single-phase pyrochlore-type La of the present invention's preparation
2Zr
2O
7Nano-powder mainly contains following steps:
(1) ZrOCl in molar ratio
28H
2O:H
2O:C
3H
7OH=1:8:10, with 5.00g ZrOCl
28H
2O slowly joins in the mixed solution of 2.24g water and 9.31g propyl alcohol, constantly stirs, and obtains clear solution A liquid; Simultaneously, La (NO in molar ratio
3)
36H
2O:H
2O:C
3H
7OH=1:2:10, with 6.66g La (NO
3)
36H
2O slowly adds in the mixed solution of 0.56g water and 9.31g propyl alcohol, constantly stirs, and obtains clear solution B liquid;
(2) A liquid and B liquid are mixed, obtain transparent mixing solutions, stir;
(3) under the condition that continue to stir, successively in mixed solution in molar ratio: citric acid: Zr
4+=0.4:1 adds citric acid 1.32g, polyoxyethylene glycol in mass ratio: Zr
4+=1:7.5 adds polyoxyethylene glycol 0.19g, and wherein, the number-average molecular weight of polyoxyethylene glycol is 20000, in molar ratio methane amide: Zr
4+=2:1 adds methane amide 1.40g, stirs 5h, obtains colloidal sol.
(4) with colloidal sol at 90 ℃ of aging 10h, then through 200 ℃ of dry 5h, obtain brown xerogel.
(5) xerogel is risen to 1200 ℃ through 10 ℃/min in retort furnace, then be incubated 1h,, with the stove cooling, obtain La
2Zr
2O
7Powder.
The present embodiment gained La
2Zr
2O
7Powder, particle size is nano level, is about 40～80nm, powder consist of single pyrrhite phase La
2Zr
2O
7
Embodiment 3
A kind of single-phase pyrochlore-type La of the present invention's preparation
2Zr
2O
7Nano-powder mainly contains following steps:
(1) ZrOCl in molar ratio
28H
2O:H
2O:C
2H
5OH=1:6:10, with 5.00g ZrOCl
28H
2O slowly joins in the mixed solution of 1.68g water and 7.14g ethanol, constantly stirs, and obtains clear solution A liquid; Simultaneously, La (NO in molar ratio
3)
36H
2O:H
2O:C
2H
5OH=1:1:10, with 6.66g La (NO
3)
36H
2O slowly adds in the mixed solution of 0.28g water and 7.14g ethanol, constantly stirs, and obtains clear solution B liquid;
(2) A liquid and B liquid are mixed, obtain transparent mixing solutions, stir;
(3) under the condition that continue to stir, successively in mixed solution in molar ratio: citric acid: Zr
4+=0.2:1 adds citric acid 0.65g, polyoxyethylene glycol in mass ratio: Zr
4+=1:5 adds polyoxyethylene glycol 0.28g, and wherein, the number-average molecular weight of polyoxyethylene glycol is 20000, in molar ratio methane amide: Zr
4+=1:1 adds methane amide 0.70g, stirs 3h, obtains colloidal sol;
(4) with colloidal sol at 80 ℃ of aging 15h, then through 120 ℃ of dry 6h, obtain faint yellow xerogel;
(5) xerogel is risen to 1200 ℃ through 5 ℃/min in retort furnace, insulation 2h,, with the stove cooling, obtain La
2Zr
2O
7Powder.
The present embodiment gained La
2Zr
2O
7As shown in Figure 4, visible gained powder is uniformly dispersed the SEM photo of powder; The present embodiment gained La
2Zr
2O
7As shown in Figure 5, the particle size of visible powder is nano level, approximately 20～80nm to the TEM photo of powder; The present embodiment gained La
2Zr
2O
7As shown in Figure 6, the phase composite of visible powder is single for the XRD spectra of powder, and structure is pyrochlore-type, and crystallinity is good.
Embodiment 4
A kind of single-phase pyrochlore-type La of the present invention's preparation
2Zr
2O
7Nano-powder mainly contains following steps:
(1) Zr (NO in molar ratio
3)
45H
2O:H
2O:C
2H
5OH=1:8:10, with 5.00g Zr (NO
3)
45H
2O slowly joins in the mixed solution of 1.66g water and 5.31g ethanol, constantly stirs, and obtains clear solution A liquid; Simultaneously, LaCl in molar ratio
36H
2O:H
2O:C
2H
5OH=1:1:10, with 2.86g LaCl
36H
2O slowly adds in the mixed solution of 0.21g water and 5.31g ethanol, constantly stirs, and obtains clear solution B liquid;
(2), with mixing such as A liquid and B liquid, obtain transparent mixing solutions, stir;
(3) under the condition that continue to stir, successively in mixed solution in molar ratio: citric acid: Zr
4+=0.1:1 adds citric acid 0.24g, polyoxyethylene glycol in mass ratio: Zr
4+=1:7.5 adds polyoxyethylene glycol 0.14g, and wherein, the number-average molecular weight of polyoxyethylene glycol is 20000, in molar ratio methane amide: Zr
4+=1:1 adds methane amide 0.52g, stirs 5h, obtains colloidal sol;
(4) with colloidal sol at 80 ℃ of aging 20h, then through 120 ℃ of dry 5h, obtain faint yellow xerogel;
(5) xerogel is risen to 1200 ℃ through 5 ℃/min in retort furnace, insulation 2h,, with the stove cooling, obtain La
2Zr
2O
7Powder.
The present embodiment gained La
2Zr
2O
7Powder, particle size is nano level, is about 20～90nm, powder consist of single pyrrhite phase La
2Zr
2O
7
Claims (7)
1. single-phase pyrochlore-type La
2Zr
2O
7The preparation method of nano-powder, realized by following steps:
(1) preparation precursor solution:
Adopt metal hydration inorganic salt as precursor, adopt the mixed solution of water and alcohol as solvent, will contain Zr
4+And La
3+Hydrated inorganic salt slowly join respectively in the mixed solution of water and alcohol, continue stirring and dissolving, obtain two kinds of precursor solutions, each component molar content ratio is respectively: Zr
4+: H
2O: alcohol=1:5～8:10, La
3+: H
2O: alcohol=1:0.5～2:10;
(2) prepare colloidal sol:
Two kinds of solution are pressed component mol ratio Zr
4+: La
3+=1:1 mixes and continues stirring, adds successively citric acid, and mol ratio is citric acid: Zr
4+=0.1～0.4:1; Add polyoxyethylene glycol, the constituent mass ratio is: polyoxyethylene glycol: Zr
4+=1:1～7.5; Add methane amide or N-METHYLFORMAMIDE, mol ratio is methane amide or N-METHYLFORMAMIDE: Zr
4+=0.1～2:1, continue to stir 1～5h with above-mentioned mixed solution, forms colloidal sol;
(3) aging:
Colloidal sol is incubated aging under 60～90 ℃, continues 10～24h, obtain wet gel;
(4) drying:
100～200 ℃ of dryings, be 5～10h time of drying, obtains xerogel with wet gel;
(5) high-temperature roasting:
Xerogel is incubated 1～5h again after the temperature rise rate of 1～10 ℃/min rises to 1000～1200 ℃,, with the stove cooling, obtains La
2Zr
2O
7Powder.
2. the described a kind of single-phase pyrochlore-type La of claim 1
2Zr
2O
7The preparation method of nano-powder is characterized in that: contain Zr
4+Hydrated inorganic salt be ZrOCl
28H
2O or Zr (NO
3)
45H
2O, contain La
3+Hydrated inorganic salt be La (NO
3)
36H
2O or LaCl
36H
2O。
3. the described a kind of single-phase pyrochlore-type La of claim 1
2Zr
2O
7The preparation method of nano-powder is characterized in that: described alcoholic solvent is methyl alcohol, ethanol or propyl alcohol.
4. the described a kind of single-phase pyrochlore-type La of claim 3
2Zr
2O
7The preparation method of nano-powder is characterized in that: described alcoholic solvent is ethanol.
5. the described a kind of single-phase pyrochlore-type La of claim 1
2Zr
2O
7The preparation method of nano-powder is characterized in that: agingly be incubated 15h under 80 ℃ of conditions.
6. the described a kind of single-phase pyrochlore-type La of claim 1
2Zr
2O
7The preparation method of nano-powder is characterized in that: dry 6h under 120 ℃ of conditions.
7. the described a kind of single-phase pyrochlore-type La of claim 1
2Zr
2O
7The preparation method of nano-powder is characterized in that: high-temperature roasting rises to 1200 ℃ with 5 ℃/min, lowers the temperature with stove after insulation 2h.
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| CN103896620A (en) * | 2014-03-11 | 2014-07-02 | 中国人民解放军国防科学技术大学 | Hierarchic porous La2Zr2O7 ceramic and preparation method thereof |
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| CN105923650A (en) * | 2016-04-20 | 2016-09-07 | 陕西科技大学 | Preparation method for nano-sized Bi2Zr2O7 powder by adopting sedimentation-calcination process |
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